US9469548B2 - Continuous hydrodynamic cavitation crystallization - Google Patents
Continuous hydrodynamic cavitation crystallization Download PDFInfo
- Publication number
- US9469548B2 US9469548B2 US15/046,941 US201615046941A US9469548B2 US 9469548 B2 US9469548 B2 US 9469548B2 US 201615046941 A US201615046941 A US 201615046941A US 9469548 B2 US9469548 B2 US 9469548B2
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- US
- United States
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- solution
- cavitation
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- crystals
- seed crystals
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- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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- 238000002425 crystallisation Methods 0.000 title claims abstract description 38
- 230000008025 crystallization Effects 0.000 title claims abstract description 38
- 239000013078 crystal Substances 0.000 claims abstract description 73
- 239000000243 solution Substances 0.000 claims abstract description 57
- 238000000034 method Methods 0.000 claims abstract description 48
- 150000001875 compounds Chemical class 0.000 claims abstract description 43
- 238000010899 nucleation Methods 0.000 claims abstract description 24
- 230000006911 nucleation Effects 0.000 claims abstract description 23
- 239000011550 stock solution Substances 0.000 claims abstract description 22
- 238000002156 mixing Methods 0.000 claims abstract description 5
- 230000035939 shock Effects 0.000 claims abstract 4
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 claims description 28
- 229910000019 calcium carbonate Inorganic materials 0.000 claims description 13
- 238000009826 distribution Methods 0.000 claims description 13
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 claims description 9
- 229910001868 water Inorganic materials 0.000 claims description 6
- 229910002092 carbon dioxide Inorganic materials 0.000 claims description 5
- 239000001569 carbon dioxide Substances 0.000 claims description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 4
- 239000000292 calcium oxide Substances 0.000 claims description 3
- ODINCKMPIJJUCX-UHFFFAOYSA-N calcium oxide Inorganic materials [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 claims description 3
- 230000015572 biosynthetic process Effects 0.000 claims description 2
- BRPQOXSCLDDYGP-UHFFFAOYSA-N calcium oxide Chemical compound [O-2].[Ca+2] BRPQOXSCLDDYGP-UHFFFAOYSA-N 0.000 claims description 2
- 230000001737 promoting effect Effects 0.000 claims 7
- 230000001939 inductive effect Effects 0.000 claims 2
- 229910010272 inorganic material Inorganic materials 0.000 claims 1
- 239000011147 inorganic material Substances 0.000 claims 1
- 238000012544 monitoring process Methods 0.000 claims 1
- 239000011368 organic material Substances 0.000 claims 1
- 230000003134 recirculating effect Effects 0.000 claims 1
- 238000004064 recycling Methods 0.000 claims 1
- 238000004519 manufacturing process Methods 0.000 abstract description 8
- 238000013461 design Methods 0.000 abstract description 2
- 239000012530 fluid Substances 0.000 description 20
- AXCZMVOFGPJBDE-UHFFFAOYSA-L calcium dihydroxide Chemical compound [OH-].[OH-].[Ca+2] AXCZMVOFGPJBDE-UHFFFAOYSA-L 0.000 description 3
- 239000000920 calcium hydroxide Substances 0.000 description 3
- 229910001861 calcium hydroxide Inorganic materials 0.000 description 3
- 239000003082 abrasive agent Substances 0.000 description 2
- 238000007792 addition Methods 0.000 description 2
- 239000012296 anti-solvent Substances 0.000 description 2
- 238000012217 deletion Methods 0.000 description 2
- 230000037430 deletion Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 229940088417 precipitated calcium carbonate Drugs 0.000 description 2
- 238000003908 quality control method Methods 0.000 description 2
- 238000009987 spinning Methods 0.000 description 2
- 238000009827 uniform distribution Methods 0.000 description 2
- 230000032683 aging Effects 0.000 description 1
- 238000010923 batch production Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000010924 continuous production Methods 0.000 description 1
- 230000001351 cycling effect Effects 0.000 description 1
- 230000029087 digestion Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000003628 erosive effect Effects 0.000 description 1
- 239000012527 feed solution Substances 0.000 description 1
- ZZUFCTLCJUWOSV-UHFFFAOYSA-N furosemide Chemical compound C1=C(Cl)C(S(=O)(=O)N)=CC(C(O)=O)=C1NCC1=CC=CO1 ZZUFCTLCJUWOSV-UHFFFAOYSA-N 0.000 description 1
- 230000000977 initiatory effect Effects 0.000 description 1
- 238000007689 inspection Methods 0.000 description 1
- 239000000543 intermediate Substances 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000005065 mining Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 230000002093 peripheral effect Effects 0.000 description 1
- 239000003208 petroleum Substances 0.000 description 1
- 238000010903 primary nucleation Methods 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 238000012552 review Methods 0.000 description 1
- 239000012047 saturated solution Substances 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000002604 ultrasonography Methods 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F11/00—Compounds of calcium, strontium, or barium
- C01F11/18—Carbonates
- C01F11/181—Preparation of calcium carbonate by carbonation of aqueous solutions and characterised by control of the carbonation conditions
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D9/00—Crystallisation
- B01D9/0036—Crystallisation on to a bed of product crystals; Seeding
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D9/00—Crystallisation
- B01D9/0081—Use of vibrations, e.g. ultrasound
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/141—Feedstock
Definitions
- This disclosure relates generally to crystallization of compounds and more particularly to the creation of seed crystals in a compound to be crystalized by subjecting a flow of the compound at high rates to cavitation in a low shear environment.
- Crystallization of compounds from solution is a separation and purification method used in the chemical, food, and pharmaceutical industries, particularly for the production of active compounds or their intermediates. Some of the goals of the crystallization process include producing a product meeting a desired purity level and also a product having the desired crystal size and size distribution. Crystallization from solution may be conducted as a batch process or as a continuous process. Batch crystallization equipment and operation is fairly simple but requires a significant investment of both time and money between batches. Additionally, batch crystallization suffers from quality control issues due to the lack of a steady state during the batch crystallization process. Continuous crystallization may be used for large volume commodity type materials with loose tolerances.
- One standard crystallization procedure involves contacting a supersaturated solution of a compound to be crystallized with an appropriate “anti-solvent” in a stirred vessel.
- the anti-solvent initiates primary nucleation which leads to crystal formation, sometimes with the help of seeding, and crystal digestion during an aging step.
- Mixing within the vessel can be achieved with a variety of agitators (e.g., Rushton or Pitched blade turbines, Intermig, etc.), and the process is done in a batchwise fashion.
- Another known crystallization procedure for homogenous fluids employs temperature variation in a solution of a compound to be crystallized in order to generate a super saturation of the compound in the solution. Crystallization can then proceed from the super saturated solution.
- an apparatus and associated method are disclosed for creating nucleation and crystallization in a flow of feed stock solution. More specifically, an apparatus and method are disclosed for crystallizing a compound using hydrodynamic cavitation induced within a cavitation zone between a spinning rotor and the outer wall (or another wall) of a cylindrical cavity or stator within which the rotor spins.
- the method includes the steps of mixing at least one stream of a feed solution of such compound to be crystallized and passing the stream through the cavitation zone between the spinning rotor and outer cavity wall of a hydrodynamic cavitation device.
- the surface of the rotor is provided with a multitude of shallow radial bores (or other cavitation producing features) and the movement of these bores induces intense cavitation events in the solution within the bores.
- the energy and pressure of the cavitation events within the flow of feed stock solution causes nucleation and the production of seed crystals. Repeat cycling of the flow through the cavitation zone of the device can cause further crystallization of the compound within the flow.
- the rotor-stator design of the cavitation device allows for high flow rates of the feed stock, the ability to subject the flow to very high energy from cavitation events, and robust service with minimized wear. Further, the device operates continuously at high flow rates making the apparatus and method of this invention suitable for crystallization of compounds within a feed stock solution at commercially desirable flow rates. Finally, the process can be tuned to provide highly reliable results to yield crystals suitable for use in industries demanding a high level of crystal size and size distribution control while still providing continuous high flow rates. The process is aided by the low shear environment of the cavitation zone, which tends to stabilize the forming nucleation seeds and crystals.
- FIG. 1 is a cut-away drawing showing an apparatus for generating nucleation and crystallization in a flow of feed stock solution according to one aspect of the invention.
- FIG. 2 is a flowchart illustrating one embodiment of the methodology of the invention.
- Embodiments of an apparatus for carrying out the methodology of the invention can take on various forms including those disclosed in U.S. Pat. Nos. 8,465,642; 8,430,968; 7,507,014; 7,360,755; 6,627,784; 5,957,122; and 5,385,298, all of which are owned by the assignee of the present invention and each of which is hereby incorporated by reference in its entirety. With the disclosures of these incorporated patents in mind, the method and apparatus of the present invention will be described generally with reference to the annexed drawing figures, wherein reference numerals indicate corresponding parts of the apparatus and steps of the method.
- FIG. 1 shows in partially cutaway and simplified fashion one embodiment of an apparatus 11 for carrying out the methodology of the present invention.
- the apparatus 11 comprises, in this exemplary embodiment, a cylindrical housing 12 formed of opposed end plates 13 joined by a cylindrical outer wall 14 , all held together with circumferential bolts 15 .
- a cylindrical rotor 16 is disposed within the housing 12 and the rotor 16 is rotatably mounted on a shaft 17 that, in turn, is journaled within appropriate bearings 18 and 19 .
- the shaft 17 is coupled to an electric motor (not shown) that, when activated, rotates the rotor within the housing at a relatively high rotation rate.
- the rotor 16 is sized such that a cylindrical space is defined between the peripheral surface of the rotor and the inside surface of the cylindrical outer wall 14 . This space is referred to herein as the cavitation zone 21 .
- a fluid inlet 22 communicates with the interior of the housing 12 on one side of the rotor 16 and a fluid outlet 23 communicates with the interior of the housing 12 on the opposite side of the rotor.
- inlets can be formed through the sides while outlets can be formed through the cylindrical outer wall, or vice versa.
- inlets and outlets are both formed through the cylindrical outer wall and preferably are oriented generally tangentially thereto.
- tangential inlets and outlets can be beneficial, particularly where a fluid being treated is abrasive.
- the tangential inlets and outlets reduce sharp turns within the fluid, which can result in erosion of surfaces within the apparatus.
- a feed stock solution containing a compound to be crystalized may be fed into the housing through the inlet 22 .
- the solution then moves to the periphery of the housing, travels through the cavitation zone 21 , and exits the housing through outlet 23 .
- the placement of the inlet and outlet is such that all of the fluid introduced through the inlet 22 must pass through the cavitation zone 21 before exiting the housing through the outlet 23 .
- the inlet may be located between rotors of a split rotor cavitator and the outlets located outboard of each of the rotors. Other configurations are possible.
- a plurality of holes or bores is formed through the outer surface of the rotor in the illustrated embodiment.
- Rotation of the rotor with a fluid present in the housing induces violent cavitation in the fluid within the bores of the rotor.
- cavitation bubbles are continuously created in fluid within the bores and continuously collapse within the bores.
- the collapsing cavitation bubbles generate intense localized shockwaves that travel from the bores through the fluid within the cavitation zone.
- the collapsing cavitation bubbles also generate heat within the fluid by exciting the molecules of the fluid. The ultimate result is that fluid within the cavitation zone is heated by the cavitation and subjected to intense shockwaves that travel throughout the fluid flowing through the cavitation zone.
- the feed stock solution can be directed from the apparatus 11 to a process tank where the seed crystals grow into larger and larger crystals through molecular attachment.
- this is not considered the most efficient and controllable technique for growing the crystals or maintaining a uniform crystal distribution.
- the feed stock solution containing the compound to be crystalized is cycled back through the apparatus 11 or a like apparatus located downstream. This both maintains a uniform distribution of seed crystals within the feed stock and promotes growth of crystals around the seed crystals by subjecting the feed stock again to the high energy environment within the cavitation zone.
- the feed stock solution can be recycled through the apparatus 11 or successive like apparatuses until the crystals entrained within the feed stock solution flow are of a desired size for a particular application and are uniformly distributed throughout the feed stock solution. In this way, the crystal size and distribution can be carefully controlled to produce crystallization of the compound within the fluid with a precision that previously has required small batch processing, but on a large and continuous scale useful in commercial production.
- FIG. 2 is a flowchart showing the steps of the present methodology in one preferred form thereof.
- a rotor-stator based cavitation device is obtained.
- One suitable device is the Shockwave Power Reactor (SPR) device available from Hydro Dynamics, Inc. of Rome, Ga.
- SPR Shockwave Power Reactor
- an appropriate feed stock solution is created or obtained with the feed stock being in liquid form and containing the compound that is desired to be crystalized.
- the feed stock is passed through the rotor-stator based cavitation device while the rotor of the device is rotated at a predetermined rotation rate. This generates the aforementioned cavitation zone and the feed stock solution containing the compound moves through the cavitation zone as it passes through the rotor-stator based cavitation device.
- nucleation of the compound is induced in the feed stock to produce seed crystals and crystallization begins to take place at the sites of the seed crystals to grow larger crystals.
- the process gradually forms crystals of the compound within the feed stock solution.
- the feed stock is examined to determine whether the crystals that have been generated are of a desired size and distribution within the feed stock solution. If not, the feed stock solution may be passed again through the rotor-stator based cavitation device to induce further nucleation and crystal growth through crystalization. Once the crystals within the feed stock solution are of a desired size and distribution, the circulation can be discontinued and the crystals can be extracted and/or used for their intended purpose.
- nucleation and crystallization is desired in an abrasive mixture or with abrasives entrained within a flow.
- Petroleum waste water and inorganics in mining are common examples, but there are many others. Initiating nucleation and crystallization in such environments is difficult or impossible with traditional techniques.
- nucleation and crystallization is easily accomplished for compounds in abrasive fluids or fluids with entrained abrasives. The ability to accomplish this can be enhanced by replacing the side inlet and outlet shown in FIG. 1 of the apparatus with inlets and outlets that inject and withdraw fluid through the cylindrical wall of the housing in a direction tangential or substantially tangential to the direction of rotation of the rotor.
- the production of Calcium Carbonate crystals was performed by mixing calcium oxide, water, and carbon dioxide to form a feed stock solution.
- the water is added to produce calcium hydroxide, and the carbon dioxide is introduced in this solution to precipitate the desired calcium carbonate, referred to in the industry as precipitated calcium carbonate (PCC).
- PCC precipitated calcium carbonate
- the calcium carbonate, water, and carbon dioxide solution was passed through a cavitation device such as that disclosed herein to form seed crystals through nucleation and the resulting solution was cycled again through a cavitation device to grow crystals of calcium carbonate around the seed crystals through crystalization.
Abstract
Description
CaO+H2O→Ca(OH)2
and
Ca(OH)2+CO2→CaCO3+H2O
The resulting crystallization was found upon inspection to have produced crystals of uniform in size and uniform distribution throughout the solution.
Claims (16)
Priority Applications (1)
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US15/046,941 US9469548B2 (en) | 2015-02-20 | 2016-02-18 | Continuous hydrodynamic cavitation crystallization |
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US201562118941P | 2015-02-20 | 2015-02-20 | |
US15/046,941 US9469548B2 (en) | 2015-02-20 | 2016-02-18 | Continuous hydrodynamic cavitation crystallization |
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US20160244334A1 US20160244334A1 (en) | 2016-08-25 |
US9469548B2 true US9469548B2 (en) | 2016-10-18 |
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Cited By (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
USD877430S1 (en) * | 2018-12-13 | 2020-03-03 | Tti (Macao Commercial Offshore) Limited | Floor cleaner |
US11155741B2 (en) * | 2015-04-24 | 2021-10-26 | Hydro Dynamics, Inc. | Method of enhancing hydration of viscosifiers using controlled mechanically induced cavitation |
USD962568S1 (en) | 2019-09-16 | 2022-08-30 | Techtronic Floor Care Technology Limited | Floor cleaner |
US11660581B2 (en) | 2020-04-30 | 2023-05-30 | Hydro Dynamics, Inc. | System and method for treatment of plants for synthesis of compounds therefrom |
US11925907B2 (en) | 2019-07-22 | 2024-03-12 | Canopy Growth Corporation | Continuous crystallization of cannabinoids in a stirred-tank reactor |
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US1758207A (en) | 1927-06-23 | 1930-05-13 | Heenan & Froude Ltd | Hydraulic heat-generating system |
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US4213332A (en) | 1979-01-15 | 1980-07-22 | M & W Gear Company | Rotor-stator configuration for water brake dynamometer |
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US5188090A (en) | 1991-04-08 | 1993-02-23 | Hydro Dynamics, Inc. | Apparatus for heating fluids |
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US9162160B2 (en) * | 2007-03-19 | 2015-10-20 | Prosonix Limited | Process for making crystals |
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2016
- 2016-02-18 US US15/046,941 patent/US9469548B2/en active Active
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US1758207A (en) | 1927-06-23 | 1930-05-13 | Heenan & Froude Ltd | Hydraulic heat-generating system |
US2283244A (en) | 1939-08-18 | 1942-05-19 | Heenan & Froude Ltd | Means for the extraction of air from the circulating water of hydraulic brakes or dynamometers |
US4213332A (en) | 1979-01-15 | 1980-07-22 | M & W Gear Company | Rotor-stator configuration for water brake dynamometer |
JPS55102491A (en) | 1979-01-29 | 1980-08-05 | Mitsutoshi Matsuoka | Continuous clarification of waste water |
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Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US11155741B2 (en) * | 2015-04-24 | 2021-10-26 | Hydro Dynamics, Inc. | Method of enhancing hydration of viscosifiers using controlled mechanically induced cavitation |
USD877430S1 (en) * | 2018-12-13 | 2020-03-03 | Tti (Macao Commercial Offshore) Limited | Floor cleaner |
US11925907B2 (en) | 2019-07-22 | 2024-03-12 | Canopy Growth Corporation | Continuous crystallization of cannabinoids in a stirred-tank reactor |
USD962568S1 (en) | 2019-09-16 | 2022-08-30 | Techtronic Floor Care Technology Limited | Floor cleaner |
US11660581B2 (en) | 2020-04-30 | 2023-05-30 | Hydro Dynamics, Inc. | System and method for treatment of plants for synthesis of compounds therefrom |
Also Published As
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US20160244334A1 (en) | 2016-08-25 |
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